materials

Article
Ultrasonic Monitoring of Setting and Strength
Development of Ultra-High-Performance Concrete
Doo-Yeol Yoo 1 , Hyun-Oh Shin 2 and Young-Soo Yoon 3, *
1 Department of Architectural Engineering, Hanyang University, 222 Wangsimni-ro, Seongdong-gu,
Seoul 04763, Korea; dyyoo@hanyang.ac.kr
2 Department of Civil Engineering and Applied Mechanics, McGill University, 817 Sherbrooke Street West,
Montreal, QC H3A 0C3, Canada; hyunoh777@gmail.com
3 School of Civil, Environmental and Architectural Engineering, Korea University, 145 Anam-ro, Seongbuk-gu,
Seoul 02841, Korea
* Correspondence: ysyoon@korea.ac.kr; Tel.: +82-2-3290-3320

Academic Editor: Jorge de Brito

Received: 22 March 2016; Accepted: 13 April 2016; Published: 19 April 2016

Abstract: In this study, the setting and tensile strength development of ultra-high-performance
concrete (UHPC) at a very early age was investigated by performing the penetration resistance test
(ASTM C403), as well as the direct tensile test using the newly developed test apparatus, and taking
ultrasonic pulse velocity (UPV) measurements. In order to determine the optimum surface treatment
method for preventing rapid surface drying of UHPC, four different methods were examined: plastic
sheet, curing cover, membrane-forming compound, and paraffin oil. Based on the test results, the use
of paraffin oil was found to be the best choice for measuring the penetration resistance and the UPV,
and attaching the plastic sheet to the exposed surface was considered to be a simple method for
preventing the rapid surface drying of UHPC elements. An S-shaped tensile strength development at
a very early age (before 24 h) was experimentally obtained, and it was predicted by a power function
of UPV. Lastly, the addition of shrinkage-reducing and expansive admixtures resulted in more rapid
development of penetration resistance and UPV of UHPC.

Keywords: ultra-high-performance concrete; setting property; early age tensile strength; ultrasonic
pulse velocity; surface treatment

1. Introduction
For several decades, concrete has been widely used in the field of civil and architectural
engineering all over the world, because of its excellent mechanical strength, durability, and economic
efficiency. However, because of some drawbacks of concrete associated with low tensile strength, low
ductility, and low strength-to-weight ratio, its application to thin-plate structures, e.g., thin walls and
long-span bridge decks, has been limited thus far. In order to overcome these drawbacks, reactive
powder concrete (RPC), which is the forerunner of the currently used ultra-high-performance concrete
(UHPC), was developed by Richard and Cheyrezy [1] in the 1990s. Since UHPC is made from a
granular mixture optimized by the packing density theory with a low water-to-binder ratio (W/B) and
since it includes a high volume content of steel fibers, it exhibits both superior strength and ductility
with a unique strain-hardening response.
However, because of the low W/B and the inclusion of high-fineness admixtures in UHPC,
the evaporation rate of water from the surface is normally too large to be replenished by bleeding.
Because of this, the surface exposed to the atmosphere dries and condenses very quickly, even while
most of the interior mortar is still fresh. This causes plastic shrinkage cracks at the surface, as well as
durability and aesthetic problems. In addition, much quicker initial and final setting times of UHPC

Materials 2016, 9, 294; doi:10.3390/ma9040294 www.mdpi.com/journal/materials

Materials 2016, 9, 294 2 of 13

are obtained when these are measured as per ASTM C403 [2], because the needle penetrates through
the condensed surface. Therefore, there is a pressing need for new ideas of appropriate methods to
prevent the rapid drying and setting of the UHPC surface.
According to a previous study [3], both free and restrained shrinkage of UHPC increase steeply at
a very early age, leading to a high possibility of shrinkage cracking. In order to predict the cracking
potential precisely, the tensile strength development needs to be investigated along with residual
stress resulting from the restraint of shrinkage. For this reason, Yoo et al. [4] developed a direct tensile
test apparatus to measure the tensile strength before the final set, based on a previous study [5].
However, it is time-consuming to measure the tensile strengths at certain times (especially at a very
early age); thus, the field application is limited. An alternative nondestructive method for determining
the strength development of concrete has been adopted by several researchers [6–10]. Because of
its many advantages (e.g., continuous measurement of microstructural change in concrete, strong
relationship between ultrasonic pulse velocity (UPV) and cement hydration, etc.), the nondestructive
method has attracted much attention from engineers for field applications. However, to the best of
the authors’ knowledge, only very limited study [4] is currently available for predicting the tensile
strength development of UHPC at a very early age using a nondestructive method.
In order to improve the shrinkage cracking resistance of UHPC, a number of restrained shrinkage
tests have been conducted by many researchers [3,11–15]. In particular, Yoo et al. [3] reported that the
cracking potential can be mitigated by selecting a lower reinforcement ratio and by using a reinforcing
bar with a lower stiffness such as a glass fiber-reinforced polymer (GFRP) bar. Park et al. [14] employed a
ring test to investigate the effect of using shrinkage-reducing admixture (SRA) and expansive admixture
(EA) on the restrained shrinkage behavior of UHPC. Based on the test results, they concluded that
the combined use of 1% SRA and 7.5% EA exhibits the best performance compared to other mixtures
such as a UHPC mixture without SRA and EA or a UHPC mixture with SRA or EA alone. Therefore,
the UHPC mixture with 1% SRA and 7.5% EA has been adopted for several structures built in Korea [16].
The effectiveness of the combined use of 1% SRA and 7.5% EA in reducing the shrinkage crack width
of UHPC slabs has also been reported by Yoo et al. [15].
Accordingly, the present study experimentally investigated the setting, tensile strength, and UPV
evolutions of two types of UHPC (with and without SRA and EA) at a very early age (before 24 h).
In order to determine the optimum surface treatment method for preventing rapid surface drying,
four different methods using plastic sheet, curing cover, membrane-forming compound, and paraffin
oil were adopted. In addition, the very early age tensile strength was evaluated by a newly developed
tensile test apparatus, and a simple power function relationship was developed to predict tensile
strength on the basis of UPV.

2. Test Program

2.1. Materials, Mixture Proportions, and Mixing Sequence

The mixture proportions used in this study are summarized in Table 1. Type 1 Portland cement
produced in Korea and silica fume produced in Norway were used as cementitious materials; their
chemical compositions and physical properties are given in Table 2. Silica sand with a grain size smaller
than 0.5 mm was used as a fine aggregate, and silica flour including 98% SiO2 with a diameter of 2 µm
was used as a filler. Coarse aggregate was not included in the mixture to improve its homogeneity.
To provide adequate workability and viscosity, 1.2% of a high performance water-reducing agent,
polycarboxylate superplasticizer (SP) with a density of 1.06 g/cm3 , was included. A W/B of 0.2 was
adopted, and in order to improve the tensile performance, 2% by volume of short straight steel fibers
with a length of 13 mm and a diameter of 0.2 mm were included. The detailed geometrical and
mechanical properties of the steel fibers are given in Table 3.
 proper fluidity and viscosity, the steel fibers were carefully dispersed and then it was mixed for an
additional 5 min. Once an adequate fluidity and viscosity for preventing the fiber segregation from
the mortar was achieved, the UHPC was cast in a mold. All test specimens were cured in a room with
a temperature of 23 ± 1 °C and a humidity of 60% ± 5% during testing.
Materials 2016, 9, 294 3 of 13
Table 1. Mixture proportions of UHPC (unit weight, kg/m3).

Steel
Silica
Table 1. Mixture proportions Silica weight, kg/m3 ).
Silica
of UHPC (unit SP
Specimen Water Cement EA SRA Fiber
Fume Flour Sand (%)
SP
(vf, %)
Steel Fiber
Specimen
UH-N Water
160.3Cement Silica Fume
788.5 197.1 Silica 236.6
Flour Silica Sand EA
867.4 - SRA - 1.2 2.0
(%) (vf %)
,
UH-A 160.3
UH-N 165.5 788.5 786.6 197.1 196.7 236.6236.0 865.3
867.4 59.0
- - 7.9 1.2 1.2 2.0 2.0
UH-A 165.5
Note: EA 786.6 admixture,
= expansive 196.7SRA = shrinkage-reducing
236.0 865.3 59.0and7.9
admixture, 1.2 2.0
SP = superplasticizer.
Note: EA = expansive admixture, SRA = shrinkage-reducing admixture, and SP = superplasticizer.
Table 2. Chemical compositions and physical properties of cementitious materials and admixture.
Table 2. Chemical compositions and physical properties of cementitious materials and admixture.
Silica Expansive
Composition % (mass) Cement
Fume Admixture
Composition % (Mass) Cement Silica Fume Expansive Admixture
CaO 61.33 0.38 13.55
CaO 61.33 0.38 13.55
Al2O3 6.40 0.25 18.66
Al2 O3 6.40 0.25 18.66
SiO2 SiO 2
21.01 21.01
96.00 96.00 3.80 3.80
Fe2 O3Fe2O3 3.12 3.120.12 0.12 - -
MgO MgO 3.02 3.020.10 0.10 - -
SO3 SO3 2.30 2.30- - 51.3551.35
K2 O - - 0.56
F-CaO K2O - - - - 16.020.56
F-CaO
Specific surface (cm2 /g) 3413 -
200,000 - 311716.02
Specific
Density (g/cm 3 ) (cm2/g)
surface 3.15 3413 2.10 200,000 2.98 3117
Density (g/cm ) 3 3.15 2.10 2.98

Table 3. Properties of straight steel fibers.

Table 3. Properties of straight steel fibers.

Aspect Tensile
Tensile Elastic
Elastic
Diameter
Diameter Length
Length Aspect Ratio Density
Density
Strength Modulus Image
df d
(mm)
f (mm) Lf (mm)
Lf (mm) (LfRatio
/df ) (g/cm3
(g/cm)3)
Strength Modulus Image
(Lf/df) (MPa)
(MPa) (GPa)
(GPa)

0.20.2 13.013.0 65.0

65.0 7.9
7.9 2500
2500 200
200

2.2. Test Equipment and Procedure

Because of its high autogenous shrinkage and cracking potential at an early age [15], the combined
use of 1% SRA and 7.5% EA has been studied by several previous researchers [14,15], and has been
2.2.1. Penetration Resistance Test (ASTM C403)
adopted for practical applications in Korea [16], as mentioned previously. Therefore, two different
mixture In proportions
order to investigate
for UHPCthe early
(i.e., aage setting
UHPC properties
mixture of UHPC,
without SRA and a penetration
EA, calledresistance
“UH-N”,test
andwas
a
performed as per ASTM C403 [2]. Since the high volume of steel fibers resist the penetration
UHPC mixture with 1% SRA and 7.5% EA, called “UH-A”) were used in this study, as given in Table 1. of the
needle, a UHPC
Glycol-based SRAmixture without
(METOLAT steel
P 860) fiber wasbyused
produced in the Chemie
Münzing present test
GmbH by simply assuming
in Heilbronn, that the
Germany
steel
and CSAfibers
EA have no effect
produced on theJapan
in Tokyo, setting properties.
(Table 2) wereIn addition, very fine silica sand, well dispersed
adopted.
For fabricating specimens, a Hobart-type laboratory mixer with 20 L capacity was used. Since
UHPC has very low W/B and no coarse aggregate, the mixing sequence was different from that for
ordinary concrete. Cement, silica fume, silica flour, and silica sand were premixed for about 10 min.
Then, water with SP was added and mixed for another 10 min. When the state of the mortar exhibited
proper fluidity and viscosity, the steel fibers were carefully dispersed and then it was mixed for an
additional 5 min. Once an adequate fluidity and viscosity for preventing the fiber segregation from the
mortar was achieved, the UHPC was cast in a mold. All test specimens were cured in a room with a
temperature of 23 ˘ 1 ˝ C and a humidity of 60% ˘ 5% during testing.
Materials 2016, 9, 294 4 of 13

2.2. Test Equipment and Procedure

2.2.1. Penetration Resistance Test (ASTM C403)

In order to investigate the early age setting properties of UHPC, a penetration resistance test was
performed as per ASTM C403 [2]. Since the high volume of steel fibers resist the penetration of the
needle, a UHPC mixture without steel fiber was used in the present test by simply assuming that the
steel fibers have no effect on the setting properties. In addition, very fine silica sand, well dispersed
in the mortar, is assumed to have insignificant implications on the setting properties. In the case of
UHPC—owing to its low W/B and high fineness admixtures—the water evaporates from the
Materials 2016, 9, 294
surface
4 of 13
faster than it can be replenished by bleeding. Thus, the exposed surface dries rapidly and condenses
evenin while most of
the mortar, is the interior
assumed cementitious
to have insignificantmatrix is still on
implications fresh. For this
the setting reason, ifInthe
properties. the penetration
case of
UHPC—owing to its low W/B and high fineness admixtures—the water evaporates
resistance test is performed without taking into account the rapid surface drying effect, the initial from the surface
fastersetting
and final than it times
can bewill
replenished by bleeding.Therefore,
be overestimated. Thus, the exposed surfacefour
in this study, driesdifferent
rapidly and condenses
surface treatment
even while most of the interior cementitious matrix is still fresh. For this
methods using a plastic sheet, a curing cover, a liquid-type membrane-forming compound, and liquidreason, if the penetration
resistance test is performed without taking into account the rapid surface drying effect, the initial and
paraffin oil were adopted, as given in Table 4. Three cylindrical plastic molds with a diameter of
final setting times will be overestimated. Therefore, in this study, four different surface treatment
150 mm and a height of 160 mm were used for each variable. The mortar surface was determined
methods using a plastic sheet, a curing cover, a liquid-type membrane-forming compound, and
by 10liquid
mm paraffin
below the top edge
oil were of the
adopted, moldinto
as given provide
Table thecylindrical
4. Three surface treatment methods.
plastic molds The needle
with a diameter
penetrated the mortar to a depth of 25 ˘ 2 mm in 10 s, and the clear distance
of 150 mm and a height of 160 mm were used for each variable. The mortar surface was determinedrule of needle impressions
was complied
by 10 mm with.below the top edge of the mold to provide the surface treatment methods. The needle
penetrated the mortar to a depth of 25 ± 2 mm in 10 s, and the clear distance rule of needle impressions
was complied with. Table 4. Surface treatment methods on casting surface.

Specimen Table 4.
Plastic Sheet SurfaceCover
Curing treatment Membrane
methods on casting
Formingsurface.
Compound Paraffin Oil
UH-N
Specimen O Sheet
Plastic O Cover
Curing O
Membrane Forming Compound O Oil
Paraffin
UH-A
UH-N XO O
O O
O OO
UH-A X O O O
2.2.2. UPV Measurement
2.2.2. UPV Measurement
Since the microstructural changes of concrete can be consistently estimated by using UPV,
Since the microstructural changes of concrete can be consistently estimated by using UPV,
several studies [6–10,17,18] have been conducted to examine the early age setting and strength
several studies [6–10,17,18] have been conducted to examine the early age setting and strength
developments in concrete
developments byby
in concrete UPVUPVmeasurement. Inorder
measurement. In ordertotomeasure
measurethethe
UPVUPV immediately
immediately after after
concrete casting,
concrete a monitoring
casting, system
a monitoring systemwas
wasimplemented asshown
implemented as showninin Figures
Figures 1 and
1 and 2. 2.

300 Transducer
100 300
Bolt

Foam rubber
220

Acrylic plate
350
100

UHPC

Acrylic plate Foam rubber

Transducer

350 350
(a) (b)
Figure 1. Schematic diagram of UPV monitoring system (unit: mm): (a) top view; (b) side view.
Figure 1. Schematic diagram of UPV monitoring system (unit: mm): (a) top view; (b) side view.
 UHPC

3
1
Acrylic plate Foam rubber

Transducer

350 350
Materials 2016, 9, 294 (a) (b) 5 of 13
Figure 1. Schematic diagram of UPV monitoring system (unit: mm): (a) top view; (b) side view.

Figure 2. Picture of UPV monitoring system.

Figure 2. Picture of UPV monitoring system.

The mold was composed of four acrylic plates with a thickness of 20 mm, and an acrylic deck.
Foam rubber was inserted between the acrylic plates and applied at the bottom surface above the
acrylic deck to prevent the propagation of signals through the molds. This is necessary because of the
fact that, since UHPC has a very low elastic modulus at an early age, the ultrasonic signals can travel
more easily through the acrylic plates than the UHPC matrix. In addition, four bolts were fastened to
assure a good contact between the used matrix and the acrylic plates. A commercial device for UPV
measurement including a function generator (Agilent 33220A, Santa Clara, CA, USA) for generating
the waveform, a filter-amplifier (Krohn-hite 3364, Brockton, MA, USA) for removing random noise
and amplifying the received signal, a digital oscilloscope (Agilent 54624A) to measure the signal,
and an ultrasonic transducer pair with a nominal frequency of 54 kHz was employed for the UPV
measurements [19]. The frequency is applicable for fresh UHPC because its UPV is slower than that of
hardened UHPC. Each ultrasonic transducer was mounted inside a circular hole at the mid-height of
the mold, and the UPV data was measured by sending a wave from the transmitting transducer into
the UHPC matrix and then receiving it with the receiving transducer. The travel time of a wave to
pass through the UHPC matrix was recorded by the digital oscilloscope, and the pulse velocity was
calculated by
Vp “ L{∆t p (1)

where Vp is the pulse velocity, L is the length of the straight wave path through the specimen, and ∆tp
is the travel time of the wave.
The digital oscilloscope measured only the longitudinal wave velocity. In addition, the
measurements started just after concrete casting, and continued for 24 h at 30 min intervals. The steel
fibers inside UHPC mortar disturb the accurate measurement of UPV; thus, a UHPC mixture without
steel fiber (identical to that used for the penetration resistance test) was adopted.

2.2.3. Direct Tensile Test

In accordance with a previous research [5], a direct tensile test apparatus was produced to measure
the very early age tensile strength of UHPC. The test apparatus and the geometry of the test mold
are shown in Figure 3. A uniaxial load was applied by a universal testing machine (UTM, Shimadzu,
Japan) with a maximum load capacity of 250 kN through displacement control at a rate of 0.8 mm/min
during testing. Since the tensile strength at a very early age (before 24 h) is extremely low, a load cell
with a maximum capacity of 5 kN and a sensitivity of 1.25 N was used up to the tensile strength of
5 kN, and after that, another load cell with a maximum capacity of 20 kN and a sensitivity of 5 N
was used. Therefore, reliable data were obtained. When the tensile strength reached almost 2 MPa
(shortly after the final set), the tensile strength was measured using a dog-bone test method, as shown
in Figure 4 [20]. The cross-section of the dog-bone specimens was 50 mm ˆ 100 mm. The alignment of
the test specimen was carefully checked using a plumb before testing. In order to improve the accuracy
of the test results, the test setup was designed with so-called pin-fixed ends to avoid secondary flexural
 0.8 mm/min during testing. Since the tensile strength at a very early age (before 24 h) is extremely
low, a load cell with a maximum capacity of 5 kN and a sensitivity of 1.25 N was used up to the
tensile strength of 5 kN, and after that, another load cell with a maximum capacity of 20 kN and a
sensitivity of 5 N was used. Therefore, reliable data were obtained. When the tensile strength reached
almost 2 MPa (shortly after the final set), the tensile strength was measured using a dog-bone test
Materials 2016, 9, 294 6 of 13
method, as shown in Figure 4 [20]. The cross-section of the dog-bone specimens was 50 mm × 100 mm.
The alignment of the test specimen was carefully checked using a plumb before testing. In order to
improve the accuracy of the test results, the test setup was designed with so-called pin-fixed ends to
stress and to assure the centric loadings. The UTM, identical to that used for very early age tensile
avoid secondary flexural stress and to assure the centric loadings. The UTM, identical to that used
strength,for very used
was under
early age displacement
tensile strength, was control at adisplacement
used under rate of 0.8 mm/min.
control at a rate of 0.8 mm/min.

100

30
70 130
30

110 70 70 70 110
430
(a) (b)
Figure 3. Schematic view of tensile test machine: (a) geometry (unit: mm); (b) test setup and failure mode.
Figure 3. Schematic view of tensile test machine: (a) geometry (unit: mm); (b) test setup and
failure mode.
Materials 2016, 9, 294 6 of 13

(a) (b)
Figure 4. Dog-bone test: (a) geometry of specimen (unit: mm); (b) test setup.
Figure 4. Dog-bone test: (a) geometry of specimen (unit: mm); (b) test setup.
After concrete casting, all the specimens were immediately covered and adhered to a plastic
sheet in order to prevent water evaporation until the testing time.
After concrete casting, all the specimens were immediately covered and adhered to a plastic sheet
in order to 3.prevent water
Test Results andevaporation
Discussion until the testing time.

3. Test Results andCharacteristics

3.1. Setting Discussionof UHPC by Penetration Resistance Test
Figure 5 shows the penetration resistance versus elapsed time curves for all test specimens. The
3.1. Settingdevelopment
Characteristics of UHPCresistance
of penetration by Penetration Resistance
was noticeably Test by the surface treatment method.
influenced
In the case of the plastic sheet, the penetration resistance was developed most rapidly; thus, the initial
Figureand5 shows the penetration resistance versus elapsed time curves for all test specimens.
final setting times were earlier than those of the other cases in Figure 5a. This is because the
The development of penetration resistance
plastic sheet was shortly removed fromwas noticeably
the surface wheninfluenced by the surface
the needle penetrated, treatment
and it caused the method.
rapid surface drying since it was exposed to the atmosphere. This led to an overestimation
In the case of the plastic sheet, the penetration resistance was developed most rapidly; thus, the initial of the
penetration
and final setting timesresistance with age.
were earlier thanOnthose
the other
of the hand,
otherthecases
use ofinaFigure
membrane-forming compoundthe plastic
5a. This is because
resulted in the slowest development of penetration resistance and the longest initial and final setting
sheet was times.
shortly removed from the surface when the needle penetrated, and it caused the rapid
This is because the membrane-forming compound easily permeated into the UHPC mortar
surface drying since
without it was and
bleeding, exposed
causedtoathe atmosphere.
delay of the settingThis led to an overestimation
development. The delay of theofstrength
the penetration
development
resistance with age. On andthepulse velocity
other hand, in the
concrete
use of at an early age has been reported
a membrane-forming compoundpreviously by
resulted in the
Kim et al. [21]. Using a curing cover or paraffin oil resulted in intermediate penetration resistance
slowest development of penetration resistance and the longest initial and final setting times. This is
development and setting times. However, because of the addition of water at the surface, the use of
because thethe
membrane-forming
curing cover delayed the compound easily permeated
setting development slightly moreinto
thanthe
the UHPC mortar
use of paraffin oil.without
Based on bleeding,
and causedthea chemical
delay ofshrinkage
the setting
test results performed by Yoo et al. [4], the paraffin oil had an insignificantand pulse
development. The delay of the strength development
effect on the cement hydration.
velocity in concrete at an early age has In addition, since paraffin
been reported oil has a lower
previously by Kimdensity (0.88
et al. g/cmUsing
[21]. 3) than
a curing
that of water and does not mix with water, it is able to prevent water evaporation without any
cover or paraffin oil resulted in intermediate penetration resistance development and setting times.
obstacle of hydration. Therefore, even though the use of a curing cover produced similar behavior to
However, that
because of the
of paraffin oil, addition of water
the use of paraffin atthe
oil on the surface,
surface the use
was chosen of most
as the the curing cover
appropriate way delayed
for the
setting development
measuring theslightly more
penetration than the
resistance use of paraffin oil. Based on the chemical shrinkage test
of UHPC.
The specimen UH-A exhibited more rapid development of penetration resistance with age,
causing earlier initial and final setting times, compared to the specimen UH-N without EA and SRA.
This is consistent with the findings from a previous study [15], and is caused by fact that the
development of setting in UHPC mortar was accelerated by the formation of large quantities of
ettringite at an early age, resulting from the use of EA. On the other hand, a more gradual increase of
penetration resistance after the initial set was obtained for UH-A than that for UH-N. The measured
Materials 2016, 9, 294 7 of 13

results performed by Yoo et al. [4], the paraffin oil had an insignificant effect on the cement hydration.
In addition, since paraffin oil has a lower density (0.88 g/cm3 ) than that of water and does not mix
with water, it is able to prevent water evaporation without any obstacle of hydration. Therefore,
even though the use of a curing cover produced similar behavior to that of paraffin oil, the use of
paraffin oil on the surface was chosen as the most appropriate way for measuring the penetration
resistance Materials
of UHPC. 2016, 9, 294 7 of 13

40
Paraffin oil Curing
Penetration resistance (MPa) cover

30 Final set (28 N/mm2)

Plastic sheet

20

Membrane
10 forming
compound
Initial set (3.5 N/mm2)
0
0 5 10 15 20
Elapsed time (hour)
(a)
40
Curing
Penetration resistance (MPa)

cover
30 Final set (28 N/mm2)

Paraffin oil
20 Membrane
forming
compound

10

Initial set (3.5 N/mm2)

0
0 5 10 15 20
Elapsed time (hour)
(b)
Figure 5. Penetration resistance versus elapsed time curve: (a) UH-N; (b) UH-A.
Figure 5. Penetration resistance versus elapsed time curve: (a) UH-N; (b) UH-A.
Table 5. Initial and final setting times.

The specimen UH-A exhibited

Specimen more
Surface rapid development
Treatment Initialof penetration
Set (hour) resistance
Final Set (hour)with age, causing
Plastic
earlier initial and final setting times, sheet
compared to the specimen8.8 UH-N without 11.5 EA and SRA. This is
Curing cover 10.2 13.2
consistent with theUH-N
findings from a previous study [15], and is caused by fact that the development of
Membrane forming compound 12.8 16.0
setting in UHPC mortar was accelerated Paraffinby
oil the formation of10.5large quantities12.8of ettringite at an early
age, resulting from the use of EA. On the cover
Curing other hand, a more gradual
5.6 increase 10.7
of penetration resistance
after the initial setUH-A Membrane
was obtained forming than
for UH-A compound
that for UH-N. 8.0 The measured 11.9
initial and final setting
Paraffin oil 5.8 10.2
times according to the surface treatment method are summarized in Table 5.
3.2. Evolution of UPV
Table 5. Initial and final setting times.
The typical ultrasonic waveforms of UH-N with paraffin oil at three different ages are shown in
Figure 6. The waveforms were measured by recording the voltage signal at the receiving transducer
with anSpecimen Surface
oscilloscope (Figure Treatment
2). Point (A) with theInitial
downward Set arrow
(Hour) Final
indicates Set (Hour)
the time when the input
pulse was first transmitted. Point sheet
Plastic (B) with the upward arrow 8.8 indicates the time when11.5 the ultrasonic
wave was received by the receiving
Curing transducer. Because
cover of the increase of stiffness
10.2 13.2 in the UHPC
mortar with
UH-N age, the travel time offorming
Membrane the ultrasonic wave was noticeably reduced as the mortar aged.
In addition, a much higher compound 12.8
dominant frequency in the waveforms was obtained at16.0the ages of 12 and
24 h, compared to that of 8 h. This is because
Paraffin oil the stiffness (penetration
10.5 resistance) of12.8
the mortar steeply
increased after about 8 h, as shown in Figure 5a; thus, the pulse velocity through the mortar
Curing
substantially increased from cover
that point. 5.6 10.7
UH-A Membrane forming
8.0 11.9
compound
Paraffin oil 5.8 10.2
Materials 2016, 9, 294 8 of 13

3.2. Evolution of UPV

The typical ultrasonic waveforms of UH-N with paraffin oil at three different ages are shown in
Figure 6. The waveforms were measured by recording the voltage signal at the receiving transducer
with an oscilloscope (Figure 2). Point (A) with the downward arrow indicates the time when the input
pulse was first transmitted. Point (B) with the upward arrow indicates the time when the ultrasonic
wave was received by the receiving transducer. Because of the increase of stiffness in the UHPC
mortar with age, the travel time of the ultrasonic wave was noticeably reduced as the mortar aged.
In addition, a much higher dominant frequency in the waveforms was obtained at the ages of 12 and
24 h, compared to that of 8 h. This is because the stiffness (penetration resistance) of the mortar
steeply increased after about 8 h, as shown in Figure 5a; thus, the pulse velocity through the mortar
substantially increased from that point.
Materials 2016, 9, 294 8 of 13
Voltage [10.0 mV/div]

(A)

(B)

Age = 8 hours
Δt = 240 μs

Time [0.5 ms/div]

(a)
Voltage [10.0 mV/div]

(A)

(B)

Age = 12 hours
Δt = 77 μs

Time [0.5 ms/div]

(b)
Voltage [10.0 mV/div]

(A)

(B)

Age = 24 hours
Δt = 29 μs

Time [0.5 ms/div]

(c)
Figure 6. Ultrasonic waveforms from oscilloscope for UH-N with paraffin oil: (a) 8 h; (b) 12 h; (c) 24 h.
Figure 6. Ultrasonic waveforms from oscilloscope for UH-N with paraffin oil: (a) 8 h; (b) 12 h; (c) 24 h.
The travel time of the ultrasonic wave in Equation (1) was obtained by subtracting the transit
time of the ultrasonic wave through the acrylic plates from the measured total time. Figure 7 shows
The travelthetime of the
evolution ultrasonic
of UPV calculated bywave in(1)Equation
Equation (1)24was
during the first h. Theobtained
shape of UPV by subtracting the transit
development
was not significantly affected by the surface treatment method, whereas the UPV values at certain
time of the ultrasonic wave through the acrylic plates from the measured total time. Figure 7 shows
ages (after an increase point) were slightly lower when a curing cover or membrane-forming
the evolution ofcompound
UPV calculated by Equation
was used compared (1)when
to the values during the
paraffin oilfirst 24 h.
was used. ThisThe shape with
is consistent of UPV
the development
results of the penetration resistance test in Figure 5. However, the use of a
was not significantly affected by the surface treatment method, whereas the UPV values at certain agesplastic sheet, which
adhered to the exposed surface immediately after casting, provided similar UPV values as those of
(after an increase point)
paraffin wereisslightly
oil, which lower
inconsistent when
with the a curing
findings from the cover or membrane-forming
penetration resistance test. This is compound
was used compared to the values when paraffin oil was used. This is consistent with the results of
the penetration resistance test in Figure 5. However, the use of a plastic sheet, which adhered to
the air-filled space in the cement paste increased [22]. This observation was more obvious in the
specimen UH-A than UH-N. Note in Figure 7 that specimen UH-A clearly exhibits an earlier starting
time for the UPV increase than its counterpart. This is caused by the accelerated setting development
at an early age, which, in turn, is caused by the large quantities of ettringite resulting from the
addition of EA. On the other hand, a more gradual increase of the UPV was observed for specimen
Materials 2016, 9, 294 9 of 13
UH-A than for UH-N, which is consistent with the penetration resistance test results. Similar UPV
values at 24 h were obtained for both UH-N and UH-A.
The values
the exposed of UPV
surface at 24 h obtained
immediately in this provided
after casting, study (approximately
similar UPV3000valuesm/s)
as were
thosequite similaroil,
of paraffin to
the UPVs
which of ordinarywith
is inconsistent cement mortar atfrom
the findings 24 h,thereported by Reinhardt
penetration resistanceettest.
al. [17].
ThisSpecifically, theplastic
is because the UPVs
corresponding
sheet to the initial
was not removed from and
thefinal setting
surface timesUPV
during (in Table 5) were
testing, found to
in contrast to be
the685 m/s
case ofand 1217 m/s
penetration
for UH-N,testing.
resistance and 1276Therefore,
m/s and 1804
it is m/s
notedforthat
UH-A,the respectively,
plastic sheet for the case for
is effective when paraffin oil
preventing waswater
rapid used.
Thus, these UPV
evaporation at thevalues
surfacecan be used
of the UHPC forsamples
determining the initial test
(i.e., mechanical andsamples,
final setting pointselements,
structural of UHPC.etc.).

4000
Plastic sheet
Ultrasonic pulse velocity (m/s)

Curing cover
Paraffin oil
3000
Membrane forming compound

2000

1000

0
0 4 8 12 16 20 24
Elapsed time (hour)
(a)
4000
Curing cover
Ultrasonic pulse velocity (m/s)

Paraffin oil
Membrane forming compound
3000

2000

1000

0
0 4 8 12 16 20 24
Elapsed time (hour)
(b)
Figure 7. Evolution
Figure of of
7. Evolution UPV in in
UPV UHPC mortar:
UHPC (a)(a)
mortar: UH-N; (b)(b)
UH-N; UH-A.
UH-A.

Figure 8 shows a schematic view of typical UPV evolution. In agreement with previous research
UPVs slightly decreased at a very early age, because when the cement was hydrated with water,
[17,18,23], an S-shaped UPV development was obtained. In stage 1, the ultrasonic wave propagated
the air-filled space in the cement paste increased [22]. This observation was more obvious in the
through the fresh UHPC mortar (a water-like viscous phase), with a relatively low UPV of
specimen UH-A than UH-N. Note in Figure 7 that specimen UH-A clearly exhibits an earlier starting
approximately 400 m/s. At the onset of the hydration process, a slight decrease of UPV was obtained,
time for the UPV increase than its counterpart. This is caused by the accelerated setting development
resulting from the increase of air-filled pores [22]. As the hydration continued, a minimum quantity
at an early age, which, in turn, is caused by the large quantities of ettringite resulting from the addition
of EA. On the other hand, a more gradual increase of the UPV was observed for specimen UH-A than
for UH-N, which is consistent with the penetration resistance test results. Similar UPV values at 24 h
were obtained for both UH-N and UH-A.
The values of UPV at 24 h obtained in this study (approximately 3000 m/s) were quite similar to
the UPVs of ordinary cement mortar at 24 h, reported by Reinhardt et al. [17]. Specifically, the UPVs
corresponding to the initial and final setting times (in Table 5) were found to be 685 m/s and 1217 m/s
for UH-N, and 1276 m/s and 1804 m/s for UH-A, respectively, for the case when paraffin oil was used.
Thus, these UPV values can be used for determining the initial and final setting points of UHPC.
Figure 8 shows a schematic view of typical UPV evolution. In agreement with previous
research [17,18,23], an S-shaped UPV development was obtained. In stage 1, the ultrasonic wave
Materials 9, 294
2016, 2016,
Materials 9, 294 10 of 13
10 of 13

of hydration products was formed and then the UPV increased sharply (stage 2). The water-saturated
propagated
porous through the fresh
solid structure wasUHPC mortar (a
continuously water-like
connected by viscous phase),products;
the hydration with a relatively
thus, the low
wavesUPV of
approximately 400 m/s. At the onset of the hydration process, a slight decrease of UPV
propagated through the solid matrix instead of through the water-like viscous phase. Accordingly, awas obtained,
noticeable
resulting from rate of increase
the increase ofofair-filled
the UPVpores
was observed
[22]. Asduring stage 2. Once
the hydration most of the
continued, pores werequantity
a minimum filled of
by hydration
hydration productsproducts, the slope
was formed of the
and thenUPVtheincrease gradually sharply
UPV increased decreased and the
(stage 2).UPV
Theconverged to
water-saturated
a constant
porous value in the
solid structure solid
was structure (stage
continuously 3).
connected by the hydration products; thus, the waves
In the case when paraffin oil was used, the inflection points tA and tB in the S-shaped UPV
propagated through the solid matrix instead of through the water-like viscous phase. Accordingly, a
evolution curves are summarized in Table 6. The specimen UH-A exhibited a much shorter time to
noticeable rate of increase of the UPV was observed during stage 2. Once most of the pores were filled
complete stage 1, owing to the acceleration of stiffness development in the mortar that included EA.
by hydration products, the slope of the UPV increase gradually decreased and the UPV converged to a
In the same manner, a faster initiation of the steep increase in the shrinkage was obtained for UH-A
constant value
(with 1% SRA in the
andsolid
7.5% structure
EA), compared(stageto3).
that for UH-N (without SRA and EA) [13].
Ultrasonic pulse velocity (m/s)

Stage 1 Stage 2 Stage 3

tA tB
Elapsed time (hour)
Figure 8. Schematic view of UPV development (UH-N with paraffin oil).
Figure 8. Schematic view of UPV development (UH-N with paraffin oil).
Table 6. Inflection points in UPV evolution curves.
In the case when paraffin oil was used, the inflection points tA and tB in the S-shaped UPV
tA tB
evolution curves are summarized inSpecimen
Table 6. The specimen UH-A exhibited a much shorter time to
(hour) (hour)
complete stage 1, owing to the acceleration of stiffness development in the mortar that included EA.
UH-N 9.8 17.2
In the same manner, a faster initiation of the steep increase in the shrinkage was obtained for UH-A
UH-A 2.0 5.1
(with 1% SRA and 7.5% EA), compared to that for UH-N (without SRA and EA) [13].
3.3. Early Age Tensile Strength Development
Table 6. Inflection points in UPV evolution curves.
The tensile strength development at a very early age is illustrated in Figure 9. Just as with the
UPV evolution, S-shaped curves were obtained
Specimen tA for both UH-N
(Hour) tBand UH-A. Before the tensile strength
(Hour)
reached approximately 2 MPa (at an applied load of approximately 14 kN), the developed tensile test
UH-N 9.8 17.2
apparatus was used (Figure 3), and after that, the dog-bone test method was adopted for measuring
UH-A 2.0 5.1
the tensile strength (Figure 4). Specimen UH-A exhibited higher tensile strength at a very early age
than UH-N did; this is consistent with the findings from the results of the penetration resistance test
3.3. Early AgeUPV
and the Tensile Strength Development
measurements. On the other hand, the tensile strengths became similar to each other at
about 24 h, which is the same trend that was observed in the case of UPV evolution. For example, the
The tensile strength development at a very early age is illustrated in Figure 9. Just as with the
average tensile strengths were found to be 6.56 MPa for UH-N and 6.45 MPa for UH-A at about 22 h.
UPV evolution, S-shaped curves were obtained for both UH-N and UH-A. Before the tensile strength
In order to predict the very early age tensile strength of UHPC with respect to UPV, the simple
reached approximately 2 MPa (at an applied load of approximately 14 kN), the developed tensile test
power function previously suggested by Pessiki and Carino [6] was adopted in this study, as follows:
apparatus was used (Figure 3), and after that, the dog-bone test method was adopted for measuring
 aVp  higher tensile strength at a very early
b
the tensile strength (Figure 4). Specimen UH-Aftexhibited (2) age
than where
UH-Nftdid;is the tensile strength (MPa), Vp is the pulse velocity (km/s), and a and b are the coefficients. test
this is consistent with the findings from the results of the penetration resistance
and the UPV
In the measurements.
current study, EquationOn (2)
thewas
other hand,
chosen the tensile
because it has astrengths became similar
simple formulation to each
and exhibits theother
at about 24 h, which is the same trend that was observed in the case of UPV evolution.
best fit with the experimental results compared to the other models suggested by Pessiki and CarinoFor example,
the average tensileand
[7] and Pessiki strengths
Johnsonwere foundare
[9], which tomost
be 6.56 MPa
widely usedforatUH-N and 6.45
the present time.MPa for UH-A at about
22 h.
Materials 2016, 9, 294 11 of 13

In order to predict the very early age tensile strength of UHPC with respect to UPV, the simple
power function previously suggested by Pessiki and Carino [6] was adopted in this study, as follows:
` ˘b
f t “ a Vp (2)

where ft is the tensile strength (MPa), Vp is the pulse velocity (km/s), and a and b are the coefficients.
In the current study, Equation (2) was chosen because it has a simple formulation and exhibits the best
fit with 2016,
Materials the experimental
9, 294 results compared to the other models suggested by Pessiki and Carino 11 of[7]
13
and Pessiki and
Materials 2016, 9, 294Johnson [9], which are most widely used at the present time. 11 of 13
The
The comparison
comparison of of tensile
tensile strength
strength and
and UPV UPV isis shown
shown in in Figure
Figure 10.10. The
The tensile
tensile strength
strength was was
increased
increased with
with the
The comparison the UPVof in
UPV exponential
tensile
in strengthor
exponential power
orandpower UPVfunction
is shown
function form. This
This is
in Figure
form. consistent
is10. The tensile
consistent with the
the findings
withstrength was
findings
from
fromPessiki
increased and
with
Pessiki and Carino
the UPV[7]
Carino [7]and
in Keating
exponential
and Keatinget
oral. [8][8]
etpower
al. forfunction
thethe
for relationship
form. This
relationship between compressive
is consistent
between with strength and
the findings
compressive strength
UPV.
from In
and UPV. addition,
Pessiki Inand the relationship
Carino
addition, the betweenbetween
[7]relationship
and Keating ettensile
al. [8]strength
for and UPVand
the relationship
tensile strength at abetween
very early
UPV age was
at compressive
a very earlyaccurately
strength
age was
predicted i.e.,function, 2 ) was found2 to be
and UPV. using
accurately In a simple
addition,
predicted thepower
using function,
relationship
a simple between
power thetensile
coefficient theofcoefficient
strength
i.e., determination
and UPV of at a(Rvery early (R
determination age) was
0.99691
found tofor
accurately UH-N
bepredicted
0.99691 and 0.96742
using
for UH-N for
andUH-A.
a simple power
0.96742 forfunction,
UH-A. i.e., the coefficient of determination (R2) was
found to be 0.99691 for UH-N and 0.96742 for UH-A.
8
8 UH-N
UH-A
UH-N by dog-bone test
(MPa)

6 UH-A by dog-bone test

(MPa)

6
strength

4
strength

4
Tensile

by developed test apparatus for

very early agetest
tensile strength
Tensile

2 by developed apparatus for

2 very early age tensile strength

0
0 0 4 8 12 16 20 24
0 Age 12
(hour)
4 16 8
20 24
Age (hour)
Figure 9. Early
Figure ageage
9. Early tensile strength
tensile development
strength (before
development 2424
(before h).h).
Figure 9. Early age tensile strength development (before 24 h).
8
8 UH-N
UH-A
UH-N
(MPa)

6 UH-A
(MPa)

6
strength

4
strength

ft = 0.249(Vp)3.057
4
ft = 0.249(Vp)3.057
Tensile
Tensile

2
2
ft = 0.146(Vp)3.478
0 ft = 0.146(Vp)3.478
0 0 500 1000 1500 2000 2500 3000 3500
0 500 Ultrasonic
1000 1500pulse 2000
velocity (m/s)
2500 3000 3500
Ultrasonic pulse velocity (m/s)
Figure 10. Relationship between early age tensile strength and UPV.
Figure 10.10.
Figure Relationship between
Relationship early
between ageage
early tensile strength
tensile and
strength UPV.
and UPV.
4. Conclusions
4. Conclusions
This study investigated the effects of the surface treatment method on the setting properties and
4. Conclusions
This study investigated
UPV evolution of two typesthe ofeffects
UHPC. of In
theaddition,
surface treatment
very early method on the strength
age tensile setting properties and
development
UPV This
(before study
evolution investigated
24 h) wasofmeasured
two types the
byof effects
UHPC.
a newly of the surface
In addition,
developed treatment
very
tensile method
testearly on the
age tensile
apparatus setting properties
strength with
and correlated and
development
the UPV.
UPV
Fromevolution
(before 24above
the ofdiscussions,
h) was two types by
measured ofthe
UHPC.
a newly Indeveloped
followingaddition, very early
tensile
conclusions age
testbe
can tensile strength
apparatus
drawn: development
and correlated (before
with the UPV.
From(1)
theThe
above
use discussions, the following
of a plastic sheet caused anconclusions
overestimationcan be drawn:
of the penetration resistance, whereas the
(1) The
addition of ause of a plastic sheet caused
membrane-forming compound an overestimation of the penetration
led to an underestimation. resistance,
The use of eitherwhereas
paraffinthe
oil
addition of acover
or a curing membrane-forming compoundvalues
resulted in intermediate led to an
withunderestimation.
behaviors that Thewereuse of either
similar to paraffin oil
each other.
or a curingthe
However, cover resulted
paraffin in chosen
oil was intermediate values
to be most with behaviors
appropriate that were
for measuring the similar to each
penetration other.
resistance
However, the paraffin
of UHPC because oillower
of its was chosen
densityto(0.88
be most appropriate
g/cm for measuring
3), its immiscibility the penetration
with water, resistance
and the fact that it
Materials 2016, 9, 294 12 of 13

24 h) was measured by a newly developed tensile test apparatus and correlated with the UPV. From the
above discussions, the following conclusions can be drawn:
(1) The use of a plastic sheet caused an overestimation of the penetration resistance, whereas the
addition of a membrane-forming compound led to an underestimation. The use of either paraffin
oil or a curing cover resulted in intermediate values with behaviors that were similar to each other.
However, the paraffin oil was chosen to be most appropriate for measuring the penetration resistance
of UHPC because of its lower density (0.88 g/cm3 ), its immiscibility with water, and the fact that it did
not interfere with hydration.
(2) The shape of UPV development with age was not affected by the surface treatment method.
In contrast, the use of a curing cover or membrane-forming compound resulted in slightly lower UPV
values at certain ages, compared to the results when paraffin oil was used. Attaching a plastic sheet to
the exposed surface was effective at preventing water evaporation, and thus, it is considered to be a
simple method for preventing the rapid surface drying of UHPC elements.
(3) The specimen UH-A (with 1% SRA and 7.5% EA) exhibited more rapid development of
penetration resistance, leading to quicker initial and final setting times, and an earlier starting time for
the steep increase in the UPV evolution, compared to those of UH-N (without SRA and EA). This is
mainly caused by the accelerated stiffness development in the UHPC mortar at an early age due to the
large quantities of ettringite that result from the addition of EA.
(4) The S-shaped tensile strength development of UHPC at a very early age (before 24 h) was
successfully measured in this study. The tensile strength increased monotonically with the UPV values
and could be accurately predicted by using a simple power function.

Acknowledgments: This research was supported by a grant (13SCIPA01) from Smart Civil Infrastructure Research
Program funded by Ministry of Land, Infrastructure and Transport (MOLIT) of Korea government and Korea
Agency for Infrastructure Technology Advancement (KAIA).
Author Contributions: Doo-Yeol Yoo and Young-Soo Yoon conceived and designed the experiments; Doo-Yeol Yoo
and Hyun-Oh Shin performed the experiments; Doo-Yeol Yoo analyzed the experimental data and wrote
the manuscript.
Conflicts of Interest: The authors declare no conflict of interest.

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